Diisopropylethylamine → 1,1-Dimethylethyl 3-methyl-4-[(1-phenyl-1H-1,2,4-triazol-3-yl)carbonyl]-1-piperazinecarboxylate

HRID 334078ノート

反応式

HRID 334078 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH:10]([CH3:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN(C(C)C)C(C)C.[C:24]1([N:30]2[CH:34]=[N:33][C:32]([C:35](Cl)=[O:36])=[N:31]2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:35]([C:32]2[N:33]=[CH:34][N:30]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[N:31]=2)=[O:36])[CH:10]([CH3:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 2756810tert-Butyl 3-methylpiperazine-1-carboxylateHCID 866882991-Phenyl-1H-1,2,4-triazole-3-carbonyl chloride

生成物 1

HCID 866883001,1-Dimethylethyl 3-methyl-4-[(1-phenyl-1H-1,2,4-triazol-3-yl)carbonyl]-1-piperazinecarboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a mixture of 2.19 g (10.5 mmol) 3-methyl-piperazine-1-carboxylic acid tert-butyl ester and 2.50 mL (14.6 mmol) DIPEA in 15 mL DCM was added a solution of 2.18 g (10.5 mmol) 1-phenyl-1H-[1,2,4]-triazole-3-carbonyl chloride in 15 mL DCM. The reaction mixture was stirred at RT for 3 days, then washed with water. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo.

後処理

  1. washwashed with water
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9aacb79db5a94d16a744a7e593cf5896
出典データセット
uspto-grants-2014_11
特許番号
US08883789B2

反応ノート

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